CN110202148B - Method for manufacturing high-entropy alloy-based multiphase reinforced gradient composite material by laser additive manufacturing - Google Patents

Method for manufacturing high-entropy alloy-based multiphase reinforced gradient composite material by laser additive manufacturing Download PDF

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CN110202148B
CN110202148B CN201910587444.2A CN201910587444A CN110202148B CN 110202148 B CN110202148 B CN 110202148B CN 201910587444 A CN201910587444 A CN 201910587444A CN 110202148 B CN110202148 B CN 110202148B
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李嘉宁
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Shandong Jianzhu University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/30—Process control
    • B22F10/36—Process control of energy beam parameters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/20—Direct sintering or melting
    • B22F10/25—Direct deposition of metal particles, e.g. direct metal deposition [DMD] or laser engineered net shaping [LENS]
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/30—Process control
    • B22F10/32—Process control of the atmosphere, e.g. composition or pressure in a building chamber
    • B22F10/322—Process control of the atmosphere, e.g. composition or pressure in a building chamber of the gas flow, e.g. rate or direction
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00—Processes of additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y80/00—Products made by additive manufacturing
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C24/00—Coating starting from inorganic powder
    • C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
    • C23C24/10—Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
    • C23C24/103—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/30—Process control
    • B22F10/38—Process control to achieve specific product aspects, e.g. surface smoothness, density, porosity or hollow structures
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

Abstract

The invention discloses a method for manufacturing a high-entropy alloy-based multiphase reinforced gradient composite material by laser additive manufacturing. Nimonic93-Zn-SiB is put in an argon environment by adopting a coaxial powder feeding method2‑CeO2The mixed powder is melted and deposited on the surface of the TA1 titanium alloy by laser to form a lower layer; then FeCoCrAlCu high-entropy alloy-TiC mixed powder is subjected to laser melting deposition on the lower layer to form an upper layer; the upper layer and the lower layer are in good metallurgical bonding and have good wear resistance. Test results show that the generation of the nanocrystalline can improve the wear resistance of the lower layer to a certain extent; the amorphous region with better toughness is also generated at the lower layer, so that the layer has strong buffer effect on friction by-products and improves the wear resistance of the gradient composite material to a certain extent. The invention can obtain the high-entropy alloy-based multiphase reinforced gradient composite material with extremely high wear resistance, and has the advantages of simple and convenient process, strong applicability, convenient popularization and application and the like. Key words: a gradient composite material; laser additive manufacturing; a titanium alloy.

Description

Method for manufacturing high-entropy alloy-based multiphase reinforced gradient composite material by laser additive manufacturing
Technical Field
The invention relates to a method for manufacturing a high-entropy alloy-based multiphase reinforced gradient composite material by laser additive manufacturing, and belongs to the technical field of material surface reinforcement. In particular to a method for preparing a high-entropy alloy-based amorphous-nanocrystalline multiphase reinforced gradient composite material on the surface of a titanium alloy by utilizing a laser melting deposition technology.
Background
The Laser Melting Deposition (LMD) technology heats and melts the powder and the surface of the workpiece through a high-energy density laser beam, and the powder and the surface of the workpiece are rapidly solidified and deposited on the surface layer by layer to form a cladding layer, so that the surface performance of the workpiece is enhanced; the LMD technology can realize the direct manufacture of the gradient composite material according to the working conditions of different parts of the workpiece. The gradient composite material can effectively relieve thermal stress caused by temperature gradient, reduce residual stress to a certain extent and further improve material performance. The amorphous-nanocrystalline material is widely applied to the aerospace field due to the characteristics of high temperature resistance, small friction coefficient, corrosion resistance and the like, and the quenching characteristic of a laser melting pool is favorable for forming amorphous-nanocrystalline and other multiple phases; the Nimonic93 high-temperature alloy has good wear resistance, toughness, thermal fatigue resistance and other properties, and is widely applied to the technical field of surface strengthening; FeCoCrAlCu high entropy synthesisThe gold (HEA) can effectively inhibit the precipitation of brittle phases in the solidification process of a laser molten pool due to the extremely high mixing entropy, and has the properties of high hardness, wear resistance, extremely strong corrosion resistance and the like. Zn can effectively promote the generation of an amorphous-nanocrystalline phase and can also perform a chemical reaction with Co in Nimonic93 in a laser melting pool to generate nano intermetallic compound particles with good performance; SiB2Is a wear-resistant and high-temperature-resistant ceramic material, and is beneficial to the generation of amorphous-nanocrystalline phase; appropriate amount of CeO2The liquidity of the liquid metal can be effectively improved, the growth directionality of the dendrite is weakened, and the laser cladding layer with uniform and compact structure is generated.
Disclosure of Invention
Based on the scientific principle, the invention provides a method for preparing the high-entropy alloy-based multiphase enhanced gradient composite material by an LMD technology according to the quenching characteristic of a high-temperature molten pool formed by laser radiation on the metal surface, and the organization structure of the prepared high-entropy alloy-based multiphase enhanced gradient composite material is shown in figure 1.
Nimonic93-Zn-SiB is put in an argon environment by adopting a coaxial powder feeding method2-CeO2The mixed powder LMD forms a lower layer on the surface of TA1 titanium alloy, a large amount of boride ceramic phase and eutectic are generated on the lower layer, and the eutectic is beneficial to generating an amorphous phase in the LMD layer (see figure 2 a); due to the quenching characteristics of the laser melt pool, many crystals have not grown long enough to solidify, forming many nanoparticles on the Nimonic 93-based LMD layer (see fig. 2 b); fig. 2c is a local TEM test result of the lower layer, demonstrating that an amorphized region is formed in the lower layer, which is beneficial for improving the wear resistance of the lower layer.
Adopting a coaxial powder feeding method to form an upper layer (a high-entropy alloy-based LMD layer) with uniform and compact tissues on the surface of the prepared lower layer by using FeCoCrAlCu-TiC mixed powder LMD in an argon environment, and distributing a plurality of granular TiC on an upper layer substrate (see figure 3 a); FIG. 3b is a top spectrum area scan analysis test area and EDS spectrum demonstrating that the lumpy precipitates are carbide strengthening phases.
The abrasion resistance of the TA1 titanium alloy surface high-entropy alloy-based multiphase reinforced gradient composite material is measured by adopting an MM200 abrasion tester; selecting the sizeΦYG6 hard alloy grinding wheel of 40X 12 mm, rotating speed 400 r/min, load 10 kg.
As shown in fig. 4, the wear volume of the prepared gradient composite material showed a significantly lower trend with the time of the test, indicating that the lower layer had a significantly higher wear resistance than the upper layer, and the wear volume of the lower layer was about TA1 substrate 1/20; the generation of the nano-crystal can improve the wear resistance of the lower layer to a certain extent; the amorphous region with better toughness is also generated at the lower layer, so that the layer generates strong buffer effect on friction pairs and improves the wear resistance of the gradient composite material to a certain extent.
The coefficient of friction (COF) of the prepared gradient composite material changes along with the contact load as shown in FIG. 5, the COF of the upper layer is more sensitive to the change of the contact load, and the COF of the upper layer is increased from 0.32 to 0.35 along with the increase of the contact load from 65N to 95N; as the contact load increased from 75N to 95N, the underlayer COF decreased from 0.35 to 0.34, indicating that the underlayer had better abrasion resistance.
Comprehensive analysis shows that the laser additive manufacturing technology is adopted, and the LMD Nimonic93-Zn-SiB on the surface of the TA1 titanium alloy is adopted to overcome the defect of poor surface wear resistance of the titanium alloy2-CeO2 Preparing a lower layer by a process method of mixed powder; then preparing an upper layer from LMD FeCoCrAlCu-TiC mixed powder on the surface of the lower layer to form a gradient composite material, thereby achieving the purpose of reinforcing the surface of the titanium alloy.
The method comprises the following specific steps:
(1) before LMD, the surface of TA1 titanium alloy is polished by No. 120 sand paper to be flat, so that the surface roughness reaches Ra 2.5 mu m; then, cleaning the surface of the titanium alloy by using a sulfuric acid aqueous solution with the volume percentage of 25%, wherein the pickling time is 5-10 min; then washing with clear water, wiping with alcohol titanium alloy, and drying;
(2) mixing Nimonic93-Zn-SiB with a certain mass ratio2-CeO2The mixed powder is LMD on the surface of the titanium alloy in a coaxial powder feeding mode to form a lower layer; then FeCoCrAlCu-TiC mixed powder LMD with a certain mass proportion is placed on the surface of the lower layer to form an upper layer; the Nimonic93 powder size is 10-150 μm, the Zn powder size is 10-150 μm, SiB2Powder size of 10-100 μm, CeO2The size of the powder is 1-50 mu m;
(3) in the upper and lower layer forming process, laser beam scans vertically and blows argon gas coaxially to protect the molten pool and the lens cone, and the technological parameters are as follows: the laser power is 1.2 kW, the scanning speed of a laser beam is 2-9 mm/s, the powder feeding rate is 30 g/min, the diameter of a light spot is 5 mm, the argon flow rate is 30L/min, the lap joint rate is 25%, and the technological methods and parameters of the upper layer and the lower layer are the same.
Step (1) the TA1 titanium alloy composition (wt.%): 0.011C, 0.035Fe, 0.001H, 0.002N, 0.038O, and the balance Ti;
step (2), mixing the powder in the following components (wt.%): 5Zn, 4SiB2，1CeO2The balance Nimonic93 (lower layer); 10TiC, the balance fecocrlcu (upper layer); chemical element components (wt.%) in Nimonic 93: 0.13C, 20Cr, 15Co, 1Al, 2Ti, 1Fe, 0.02B, 0.8Mn, 0.8Si, 0.015P, 0.015S, 0.2Cu, 0.0025Pb, and the balance of Ni; the molar mass of each element of the FeCoCrAlCu powder is the same.
According to the invention, LMD treatment is carried out on the surface of a titanium alloy sample in an argon environment, then laser is turned off, and argon protection is turned off after 2-3 seconds, so that the sample is fully protected by protective gas, and the high-entropy alloy-based multiphase reinforced gradient composite material with extremely high wear resistance can be obtained. The invention has the advantages of simple and convenient process, strong applicability, convenient popularization and application and the like.
Detailed description of the preferred embodiments
Example 1:
cutting the TA1 titanium alloy into cuboid samples of 10 mm multiplied by 25 mm, cleaning the surface of the titanium alloy before LMD, wiping clean and drying; mixing 90Nimonic93-5Zn-4SiB2-1CeO2(wt.%) mixed powder LMD formed a lower layer on TA1 titanium alloy 10 mm × 25 mm surface, and then 90 fecocrlcu-10 TiC (wt.%) mixed powder LMD was placed on the lower layer to form an upper layer.
The specific process steps are as follows:
(1) before LMD, the surface of TA1 titanium alloy is polished by No. 120 sand paper to be flat, so that the surface roughness reaches Ra 2.5 mu m; then, cleaning the surface of the sample by using a sulfuric acid aqueous solution with the volume percentage of 25%, wherein the pickling time is 5-10 min; then washing with clear water, wiping the surface of the sample with alcohol, and drying;
(2) respectively weighing 90 g of Nimonic93 powder, 5 g of Zn powder and SiB by using an electronic balance2Powder 4 g, CeO21 g of powder, and placing into a No. 1 beaker; weighing 90 g of FeCoCrAlCu powder and 10 g of TiC powder by using a balance, and putting the powder into a No. 2 beaker, wherein the size of Nimonic93 powder is 100 mu m, the size of Zn powder is 100 mu m, and SiB2Powder size 50 μm, CeO2The powder size is 10 μm;
(3) directly blowing the mixed powder in the No. 1 beaker to the surface to be processed of the sample by using a coaxial powder feeding device to carry out LMD (laser melting) to form a lower layer; the technological parameters are as follows: the laser power is 1.2 kW, the scanning speed of a laser beam is 4 mm/s, the powder feeding speed is 30 g/min, the diameter of a light spot is 5 mm, the lap joint rate is 25%, and the argon flow speed is 30L/min;
(4) blowing the mixed powder in the beaker 2 to the lower layer surface by using a coaxial powder feeder to carry out LMD so as to form an upper layer; the technological parameters of the upper layer are the same as those of the lower layer prepared before, and argon is also used as protective gas.
Description of the figures
FIG. 1 is a structural structure of a high-entropy alloy-based multiphase reinforced gradient composite material
FIG. 2 (a) lower layer microstructure, (b) nanoparticles formed in the lower layer, (c) lower layer TEM test
FIG. 3 (a) upper layer microstructure, (b) upper layer energy spectrum area scan analysis region and its results
FIG. 4 is a graph of the wear volume of an LMD gradient composite material as a function of time
FIG. 5 distribution diagram of the change of the LMD gradient composite material COF with the load

Claims (1)

1. A method for manufacturing a high-entropy alloy-based multiphase reinforced gradient composite material by laser additive manufacturing is characterized by comprising the following steps of:
(1) mixing Nimonic93-Zn-SiB with a certain mass ratio2-CeO2Fully mixing and drying the mixed powder; then Nimonic93-Zn-SiB is put in a coaxial powder feeding device2-CeO2The mixed powder is blown to the surface of TA1 titanium alloy to carry out laser melting deposition to form a lower layer, laser beams are adopted to vertically scan and coaxially blow argon to protect a molten pool and a lens barrel, and the process parameters are as follows: the laser power is 1.2 kW,the scanning speed is 2-9 mm/s, the powder feeding speed is 30 g/min, the diameter of a light spot is 5 mm, the argon flow speed is 30L/min, and the lap joint rate is 25%; the lower layer mixed powder comprises the following components in percentage by mass: 5Zn, 4SiB2，1CeO2The balance being Nimonic 93; the mass fraction of each chemical element component in Nimonic93 is as follows: 0.13C, 20Cr, 15Co, 1Al, 2Ti, 1Fe, 0.02B, 0.8Mn, 0.8Si, 0.015P, 0.015S, 0.2Cu, 0.0025Pb, and the balance of Ni;
(2) fully mixing FeCoCrAlCu-TiC mixed powder in a certain mass ratio and drying; then blowing FeCoCrAlCu-TiC mixed powder to the lower layer surface by using a coaxial powder feeding device to carry out LMD to form an upper layer; laser beam vertical scanning and coaxial blowing argon protection molten pool and lens cone, process parameters: the laser power is 1.2 kW, the scanning speed is 2-9 mm/s, the powder feeding rate is 30 g/min, the spot diameter is 5 mm, the argon flow rate is 30L/min, and the lap joint rate is 25%; the mass fraction of the upper layer mixed powder component is as follows: 10TiC and the balance FeCoCrAlCu; the molar mass of each element of the FeCoCrAlCu powder is the same.
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